In several points of rivers Toksa, Neva and water objects related to them chemical analysis of water was done, optical density at 254 nm (OD254) and SUVA254 were determined. Tributaries of the Toksa polluted by domestic wastewaters showed values increased several fold (compared to the Toksa waters) for: colour, OD254, TOC, electric conductivity (EC), concentrations of ammonium (up to 10 maximal allowable levels for surface waters) and chlorides. SUVA254 (in L/(mgTOC·m)) belonged to the following ranges: 1.8-3.0 in the Toksa and its source; 2.3-6.3 in its polluted tributaries; 2.7-3.5 in the Neva and its source; 2.1-2.6 in the tap water of St. Petersburg. For express control of the pollution in the Toksa and other rivers with similar properties measurement of EC and OD254 could be recommended. Control of organic matter content based solely on OD254 cannot be precise due to variations of SUVA254.